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1 Name Date Grade Pre- Lab Questions: Synthesis and Crystallization of Alum MUST be completed before an experiment is started. Show all work and be sure to include units. Q1. Based on the general chemical formula of an alum, give formulas for three different alums. Q2. If 25 students perform this experiment in a laboratory, and each student begins with 3.00 g of aluminum, (a) How many moles of H 2 gas are produced by each student? (b) What volume of H 2 gas is produced by each student at STP? (c) What total volume of H 2 gas is produced in the laboratory? (d) If the laboratory dimensions are 12 m x 10 m x 4 m, what is the volume of the laboratory in liters? (1 m 3 = 1,000 L) (e) A concentration of more than 10 volume percent of H 2 gas in air is explosive when ignited. Is it safe for all 25 students to carry out the dissolution of aluminum at the same time? Would it be safe if each student used 1.00 kg? CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 1

2 Q3. If the starting weight of aluminum in grams is the sum of the last three numbers in your student ID divided by 10, (a) What is the theoretical yield of alum in grams from this starting weight? Starting weight Theoretical yield (b) What is the minimum volume of 1.5 M KOH that will be required to dissolve this weight of aluminum? Q4. Potassium salts are much more expensive than ammonium salts. Ammonium aluminum alum can often be used interchangeably with potassium aluminum alum. What is the maximum weight of ammonium aluminum alum that can be made from 2.20 g of aluminum? Q5. Aluminum foil includes a small amount of iron. Suppose we choose to dissolve the aluminum in acid instead of base as the first step of synthesis. Describe the steps of this synthesis. Can you suggest any advantages or disadvantages to this synthetic pathway? CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 2

3 Purpose Experiment I: Synthesis and Crystallization of Alum The purpose of this experiment is to 1) synthesize crystals of potassium aluminum sulfate dodecahydrate and 2) calculate the percent yield of the product during this synthesis. Introduction Alums are a class of double sulfates (salts containing the SO 4 2- anion) in which one cation is monovalent and the second cation is trivalent. The general chemical formula of an alum is M(I)T(III)(SO 4) 2 xh 2O, where M(I) represents the Monovalent cation (most often potassium (K + ), sodium (Na + ), ammonium (NH 4 + ), etc.), and T(III) the Trivalent cation (most often aluminum (Al 3+ ), but also Iron (Fe 3+ ), Chromium (Cr 3+ ), etc.) and x, the number of moles of water of crystallization is usually equal to 12. The most common form of alum is potassium aluminum sulfate, called potassium aluminum alum or just plain alum, KAl(SO 4) 2.12H 2O. The full chemical name of this substance is potassium aluminum sulfate dodecahydrate. This material occurs naturally as the mineral called alum. Aluminum is the third most abundant element in the earth s crust. The metal and its salts are used extensively in everyday chemical processes. Alum has been used by humans for centuries. It is used in industry as a clarifier (in water purification), in the manufacturing and application of dyes, in the tanning of leather, in marble and porcelain cements, and medicinally as an astringent (a substance that draws together or constricts tissues) and styptic (to control bleeding). Alum has found extensive application in the paper industry as a sizing agent (a material that fills the spaces between the paper fibers to control its porosity and to bind other additives). Unfortunately, the acidity of the aqueous Al 3+ ion makes the paper mildly acidic and, therefore, contributes to its disintegration over the long term. Chemical processes that neutralize this acidity are currently in use in major libraries. Alum has also played a major role in economic history. The mixed alum of K +, Al 3+, and Fe 3+ was isolated from its natural deposits during the Roman Empire. Alum itself was prepared commercially in chemically pure form in Turkey in the 13 th century and continuously, since 1450, near Rome from a related mineral, alunite (or alumstone). The process was similar to that described in this exercise. Aluminum is an active metal that dissolves in strong acids and in strong bases. It does not seem like an active metal in everyday use because it forms a tightly bound oxide coat on its surface that protects it from further oxidation. In the first step of today s lab, you will dissolve aluminum in a potassium hydroxide solution according to the following chemical equation: Reaction 1: 2Al (s) + 2KOH (aq) + 6H 2O (l) à 2KAl(OH) 4 (aq) + 3H 2 (g) The substance KAl(OH) 4 consists of a K + ion and the aluminate ion, Al(OH) 4. The four hydroxides in the aluminate ion are arranged around the Al with tetrahedral geometry, pointed towards the corners of a four- sided pyramid. In the second step of this experiment, you will observe the reaction between potassium aluminate and sulfuric acid: Reaction 2: KAl(OH) 4 (aq) + 2H 2SO 4 (aq) à KAl(SO 4) 2 (aq) + 4H 2O (l) The acidic hydrogens in the sulfuric acid form water as they strip off and react with the OH ions bound to the aluminum in the aluminate ion. The Al 3+ ion, now free of the OH ions, becomes surrounded by 6 water molecules, arranged around the aluminum ion with octahedral geometry like the xyz- axes of a Cartesian coordinate system. The Potassium ions are also surrounded (hydrated) by 6 water molecules. CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 3

4 As the potassium aluminum sulfate solution cools, crystals of KAl(SO 4) 2 12H 2O form. The 12H 2O in the formula indicates that these 12 water molecules are coordinated within its structure. The raised dot before the water formula is used to show that this is a hydrate, that is, a crystal that has water molecules as an integral part of the crystal. When calculating molecular masses, the mass of water in a hydrate must be included. As previously described, KAl(SO 4) 2 12H 2O is one of many compounds classified as alums. A mono- positive ion and a tri- positive ion bound to two (2) sulfate ions, with twelve (12) water molecules of hydration, identify the alums. The mono- positive ion is usually from group 1 of the periodic table, and the tri- positive ion is usually aluminum, gallium, indium, vanadium, chromium, iron or cobalt. The aluminum family alums are colorless, while the transition metal alums are colored. You will use an aluminum can as the source of aluminum. This is not recycling, since the major cost in producing aluminum is the cost of the electricity needed to get aluminum from its ionic state into its metallic state. Rather, you will use the can, which usually holds a cool beverage, to make cool crystals of alum. In this lab, you will also be using two techniques for filtration; gravity filtration and vacuum filtration. The detailed explanation is given in the experimental procedure section. Experimental Procedure Safety Considerations for this experiment: 1. You will be using 1.4 M KOH and 9M H 2 SO 4 solutions in this lab. Handle these chemicals with care. 2. When cutting piece of aluminum metal, hold the metal piece with tongs. 3. Do not touch the hot beakers with bare hands. Use tongs. 4. Do not leave the hotplate or the hot water bath unattended. 5. Be sure to wear your safety goggles and lab apron at all times. 6. Clean all glassware used for the experiment before leaving the laboratory. 7. Waste must be disposed off in appropriate containers. 8. Wash your hands before leaving the lab room. Experiment This experiment will involve: 1. Synthesizing crystals of potassium aluminum sulfate dodecahydrate. 2. Calculating the % yield of alum formed during this synthesis. CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 4

5 Procedure There are several steps to this experiment. The procedure is given in detail below: Step 1: Prepare the aluminum sample: 1. You will be using a piece of aluminum obtained from an aluminum can. 2. Set the aluminum on a piece of scrap paper so you do not scratch the lab table, and clean off the painted surface of aluminum metal by vigorously rubbing with sand paper. 3. The inside of the aluminum can is painted with a clear varnish, so scour it as well. Cut any still- painted edges off, as it is hard to clean around the edges. 4. Rinse and dry the cleaned aluminum with DI water. 5. Make many parallel cuts along one edge (like making a hula skirt from construction paper), and then cut it into tiny confetti- sized pieces (about 2 mm square) onto some dry paper towel. 6. Zero out a sheet of weighing paper on a balance, and weigh between 0.40 and 0.60 grams of the aluminum. Record the mass of aluminum in data record sheet. Step 2: Setting up a gravity filtration apparatus 1. Set up a gravity filtering apparatus as shown in Figure I below. 2. Obtain a large size round filter paper, and fold into a cone as shown in Figure 1(b). 3. Insert filter paper into the funnel and moisten the paper with DI water. Pour off excess water. 4. Press the paper into the funnel to give it a tight fit. 5. Set the funnel on a funnel support over a 150 ml beaker. (a) Fold filter paper to half and then to a quarter length (b) Pull 3 layers to one side to make a cone (c) Insert the filter paper into the funnel. Moisten the paper with small amount of DI water. Pour off excess water. Press the paper into the funnel to give a tight fit. (d) Set the funnel on a funnel support over a 150 ml beaker Figure I : Setup for Gravity Filtration CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 5

6 Step 3: Reaction of Aluminum to form Potassium Aluminate 1. Obtain a 150- ml beaker. This beaker is different from the one that you used for the filtering setup. 2. Mark your initials in the white square of the beaker. Transfer the aluminum prepared in Step 1 into this beaker. 3. The remaining parts in this step will be completed under the fume hood. 4. Add 25 ml of 1.4 M KOH and place the beaker on the hot plate at low setting. Stir occasionally. 5. Make sure you know which beaker is yours, and be careful of other student s beakers when you stir yours. No more than 3 or 4 beakers should be on any one hotplate. 6. The aluminum will fizz as hydrogen gas is given off. The solution will turn dark from bits of paint and alloying elements in the aluminum can. 7. All of the aluminum should dissolve in 10 to 20 minutes. Step 4: Reaction of Potassium Aluminate to form Potassium Aluminum Sulfate 1. While still working under the hood, use beaker tongs to bring the beaker from Step 3 onto a fiberglass pad. 2. The last person to remove their beaker from hot plate should turn off the hot plate. Hot plate will be used again in Step SLOWLY and CAREFULLY add 10 ml of 9 M H 2 SO 4 to the contents of the beaker. As you add the acid, heat is given off which causes the solution to boil up. Be prepared for this; take time and care in pouring small portions of acid in the beaker. 4. Stir the mix, grasp the beaker with the beaker tongs, and carefully navigate back to your lab work area where you have the filtering apparatus set up. 5. Moisten the filter paper on the funnel with a small amount of the solution. Then Pour the hot solution into the filter paper in the funnel. The volume is such that it should comfortably fit, but make sure that you don t overfill the funnel. 6. The filtrate exiting the funnel should be clear and colorless. 7. When contents of the beaker have been filtered, transfer the filtrate into a clean and dry 50- ml beaker. 8. Dispose of filter paper from this step in the trash can. Step 5: Cooling the Filtrate 1. Fill one third of a 400- ml beaker with ice. 2. Add water to just under the level of ice. 3. Carefully set the beaker with the filtrate into the ice- bath. 4. Stir the filtrate occasionally. Be careful that you don t get water from the ice bath into the beaker with the filtrate. 5. You should see the solution turn cloudy in a few minutes. Stir a few times a minute. When the filtrate is milky white and ice cold, you are ready for a second pressure- assisted filtration using a Büchner funnel. CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 6

7 Step 6: Vacuum Filtration 1. Place the smaller size filter paper into the Büchner funnel. It should fit exactly inside the funnel. 2. Moisten it with deionized water, pouring off excess water. Firmly insert the funnel into the filter flask. Secure the filter flask using clamps. 3. Connect the filter flask to the water aspirator using thick tubing, and make sure that the water aspirator is drawing a vacuum. Check with your instructor to be sure that your setup is correct. See Figure 2 below for the correct setup of vacuum filtration apparatus. 4. Stir the contents of the beaker from Step 5 thoroughly, and then quickly pour the entire contents into the Büchner funnel. You should see clear liquid running out from the Büchner funnel into the filtering flask. 5. When all of the liquid has run into the filter flask, the filter paper inside the Büchner funnel should have a nice fine white residue on it. Pour 5 ml of methanol into the funnel. 6. After it has filtered through, repeat with another 5 ml of methanol. These rinsing remove excess water and sulfuric acid from the crystals. Keep the aspirator going for 5 to 10 minutes so that all the liquid runs into the filtering flask. The air forced through the funnel will also evaporate methanol from the crystals. 7. During this time, you should clean up your area, but do not leave your experiment unattended. 8. After 5 to 10 minutes, turn off the water aspirator. 9. Unplug the filter flask from the water aspirator. 10. Remove the Büchner funnel from the filter flask. Figure 2: Setup for Vacuum Filtration Step 7: Determining Mass of Alum Crystals from First Crystallization 1. Weigh a clean and dry 50- ml beaker and record the weight on the data record sheet. 2. Slam the top portion of the Büchner funnel face down onto this beaker to release the solid from the funnel. Spread the powdery crystals in the beaker to dry for 10 minutes. 3. While the powdery crystals are drying, dispose of the liquid in the filtering flask, and the filter paper into the appropriate waste container. 4. After the 10 minute drying time, weigh and record the weight of the beaker containing alum into the data record sheet. Show these crystals to your instructor. Your instructor will make note of the appearance on the data sheet. CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 7

10 Post- Lab Questions: Synthesis and Crystallization of Alum Please answer the following questions and show all work and units. Express all answers to the correct number of significant digits. All completed questions must be submitted with your lab report. Q1. How many moles of KOH were used in Step 3 of this experiment? (Refer to the volume and molarity information given in the experimental procedure.) Q2. In reaction 1, how many moles of KOH reacted with the amount of Al that you used? Q3. Given that the aluminum was limiting, how many moles of KOH were left over? Q4. How many moles of H 2 SO 4 were added in step 4 of this experiment? (Refer to the volume and molarity information given in the experimental procedure.) Q5. In reaction 2, given that KAl(OH) 4 was limiting, how many moles of H 2 SO 4 were actually used to form the maximum possible amount of KAl(SO 4 ) 2? How many moles of H 2 SO 4 were leftover? CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 10

11 Q6. Some of the excess H 2 SO 4 also reacted with the excess KOH leftover from reaction 1. The reaction produces potassium sulfate and water. Write the balanced acid- base neutralization reaction between sulfuric acid and potassium hydroxide. Q7. Calculate how many moles of H 2 SO 4 were required to react with the leftover KOH calculated in Q3. Q8. From the amounts of H 2 SO 4 calculated in questions Q4, Q5, and Q7, how much H 2 SO 4 is in excess? Q9. If you had added sodium bicarbonate, NaHCO 3, to neutralize the excess H 2 SO 4. The reaction would produce sodium sulfate, water, and carbon dioxide. Write the balanced reaction equation and include the states of matter. Q10. Calculate how many grams of sodium bicarbonate required for this neutralization reaction. CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 11

12 Q11. Assume that you used exactly 50. ml of 1.5 M KOH, 20. ml of 9.0 M H 2SO 4, and the same mass of aluminum from your experiment. If the reaction solution (before crystallization) contains theoretical yield of alum, what other substance(s) is/are in the final solution and at what concentration(s)? Q12. What factors in this experiment might contribute to an actual yield of less than 100%? CHEM- 01A - Experiment I: Synthesis and Crystallization of Alum 12

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